[go: up one dir, main page]

EP0028713A1 - Matting agent for varnishes based on wax, process for its production, and matted varnishes - Google Patents

Matting agent for varnishes based on wax, process for its production, and matted varnishes Download PDF

Info

Publication number
EP0028713A1
EP0028713A1 EP80106157A EP80106157A EP0028713A1 EP 0028713 A1 EP0028713 A1 EP 0028713A1 EP 80106157 A EP80106157 A EP 80106157A EP 80106157 A EP80106157 A EP 80106157A EP 0028713 A1 EP0028713 A1 EP 0028713A1
Authority
EP
European Patent Office
Prior art keywords
wax
weight
matting agent
varnishes
amide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP80106157A
Other languages
German (de)
French (fr)
Other versions
EP0028713B1 (en
Inventor
Karl Dr. Petz
Klaus Dr. Rieger
Dieter Steidl
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hoechst AG
Original Assignee
Hoechst AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hoechst AG filed Critical Hoechst AG
Publication of EP0028713A1 publication Critical patent/EP0028713A1/en
Application granted granted Critical
Publication of EP0028713B1 publication Critical patent/EP0028713B1/en
Expired legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/42—Gloss-reducing agents

Definitions

  • waxes of different compositions for leak matting has been known for many years (Handbook of Nitrocellulose Varnishes, Kraus, Part 2, page 116, Soaps - Oils - Fats - Waxes, 102nd Year No. 6/1976, page 163) .
  • the waxes had to be melted and by incorporating them into the lacquer or the solvent and cold stirrer, free-flowing dispersions or paste-like preparations were obtained, with which the lacquers could then be matted in the desired manner. This process was time consuming and risky in terms of a fire hazard.
  • micronized hydrocarbon waxes have been on the market for a number of years, and have proven themselves due to their ease of incorporation without the aid of heat (essay "Matting agents for paints” in “Adhesion”, November issue 1977; “Paints and solvents”, Verlag Chemie , Page 15).
  • a combination with matting agents on an inorganic basis is quite common.
  • wax-like mottling agents has shown that especially high-quality polyethylene vinegar powders with a particle size distribution in the range of 10 to 15 microns as an upper limit can best meet the requirements set by the paint industry and are superior in some respects to matting agents with different compositions.
  • Such very fine powders are e.g. B. described in DS-OS 2,713,550.
  • They consist of a ternary mixture of polyolefin wax an ester wax or a partially saponified ester wax and a diester of a monocarboxylic acid with a diol or a monocarboxylic acid diamide and are adjusted to a particle size distribution of 60 to 80% between 1 to 15 microns by spraying the mixed wax mixture and subsequent screening.
  • polyolefin waxes can then be easily comminuted to the desired fineness by grinding if hard and brittle amide wax is added during the grinding.
  • the invention therefore relates to a process for producing a wax matting agent based on wax with a particle size distribution of 99% by weight ⁇ 15 microns, which is characterized in that a polyolefin wax with an average molecular weight of 1,000 to 9,000 and an amide wax with a flow / Dropping point of 130 to 150 ° C in a weight ratio of 90: 10 to 10: 90 is subjected to a common grinding.
  • lacquer matting agent souie lacquers produced by this method which contain such lacquer matting agent.
  • the amide wax content in the matting agents hardly contributes to the matting effect, but surprisingly supports the effects of the matting component on the lacquer surface by improving the sliding effect and the resulting insensitivity to scratches. This was by no means predictable. Rather, it had to be assumed that the amide wax would only function as a grinding aid and that its presence, at least at higher concentrations, would prove to be disadvantageous with regard to paintability and adhesion.
  • Polyolefin waxes which are a constituent of the matting agents according to the invention, are monomers and copolymers of ethylene, propylene and butylene with melting intervals in the range from 90 to 140 ° C. and an average molecular weight of 1,000 to 9,000, preferably 2,000 to 4,000 . Ethylene-propylene copolymers with predominant ethylene-tooil are preferred.
  • Suitable amide waxes are reaction products of technical fatty acids with 12 to 34, preferably 12 to 18 carbon atoms with bivalent aliphatic amines with 2 to 6 carbon atoms, such as.
  • the pour / dropping points from 130 to 150, preferably 140 to 145 ° C.
  • a preferred amiduach is di-steaorylethylondiamide.
  • the grinding is carried out in such a way that the two wax components in powder, granule or flake form are either already mixed or, advantageously, fed to the mill side by side.
  • the weight ratio of polyolefin wax to amide wax is 90:10 to 10:90, preferably 70:30 to 30:70 and in particular 60:40 to 40:60.
  • the fine powder obtained according to the invention can be cold worked into the coating systems to be matted with the usual stirrers or dissolvers.
  • the desired matt effect which, as already mentioned, is essentially determined by the proportion of polyolefin wax in the mixture
  • Higher matting additives are necessary for pigmented paints.
  • Predispersion in the solvents used can accelerate the distribution in the paint.
  • a counterflow impact mill which consists of a grinding zone and an integrated wind sifter, is fed with 250 kg of an Uachs mixture per hour.
  • the wax mixture is a rough 1: 1 mixture of spray-finished distearoyl-ethylenediamide with particle sizes ⁇ 400 / u and a cut-granulated polyethylene wax (build-up polyethylene wax with a molecular weight of approx. 3,000, dropping point 122 to 127 ° C) with edge lengths of 2 to 4 mm.
  • the product is fed into the air classifier via a dosing screw. From there, the particles, which do not meet the fineness requirements, enter the grinding zone through two opposing injectors operated with compressed air. They collide head-on and are thereby micronized.
  • the ground material emerging from the mill is pneumatically discharged into a silo with a ventilation filter using the air flow.
  • the compressed air requirement at this throughput is 34 Nm 3 / min at 7 bar and 20 ° C.
  • the rotor speed of the classifier is set at 4,000 rpm. After a start-up time of approx. 15 minutes, the 1: 1 mixing ratio of the grinding components has set in the millbase leaving the mill. According to the Coulter Counter Analysis, the ground product has a weight distribution of over 99% less than 14 / u and 50% less than 4.5 / u.
  • Example 1 69 kg / h of the liquid mixture used in Example 1 are introduced into a mechanical classifier mill with a vertical axis via a metering screw.
  • the mill is a combination of a beater mill with a paddle wheel viewer. It is equipped with a tangential material entry and a fresh air intake duct.
  • the near the mill speed of 4000 rpm -1, the classifier speed of 2200 rpm - m] 1 and with an air throughput of 3100 3 / h from the mill discharged fine material has a particle size distribution of 99.5% ⁇ 14.3 / u .
  • the 50% limit is 6.0 / u.
  • a moisture-curing polyurethane varnish with a solids content of 42% (Beckacoat PU 428 from HOECHST AG) is matted as indicated in Example 3 with the fine powder obtained according to Example 1.
  • the matt lacquer film cannot be polished.
  • An acid-curing paint with a solids content of 40% (Beckurol HP 310 from HOECHSTAG), to which 1 part of p-toluenesulfonic acid, dissolved in 19 parts of n-butanol, is added as a hardener to 100 parts of paint, is matted with the polyethylene wax fine powder according to Example 1 .
  • the paint films are tested as indicated in Example 3. They cannot be polished.
  • the coating films were tested as indicated in Example 3. The films cannot be polished.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Lubricants (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Polymerisation Methods In General (AREA)
  • Paper (AREA)

Abstract

The invention provides a process for the manufacture of a polyethylene wax micro-powder, 99 weight % of which has a grain size of less than 15 microns, for the dulling of varnishes. Such a micro-powder generally cannot be obtained without difficulty by grinding; in accordance with the invention this is possible, however, by grinding the polyethylene wax together with an amide wax.

Description

Durch Einarbeitung fester Stoffe in sehr feiner Verteilung in AnEtrichrnitteln erhält man Systeme, die das einfallende Licht diffus streuen. Der Brechungsindex des zugesetzten Mattiorungsmittels soll demjenigen des Bindemittels nahekommen, so daß die Anwesenheit des Mattierungsmittels im Lackfilm bei durchfallendem Licht praktisch nicht zu erkennen ist.By incorporating solid substances in a very fine distribution in paint screeds, systems are obtained that diffuse the incident light. The refractive index of the matting agent added should come close to that of the binder, so that the presence of the matting agent in the lacquer film is practically invisible when the light shines through.

Neben anorganischen Mattierungsmitteln ist die Verwendung von Wachsen unterschiedlicher Zusammensetzung zur Leckmattierung seit vielen Jahren bekannt (Handbuch der Nitrocelluloselacke, Kraus, Teil 2, Seite 116, Seifen - Öle - Fette - Wachse, 102. Jahrg. Nr. 6/1976, Seite 163). Üblicherweise mußten die Wachse aufgeschmolzen werden und durch Einarbeiten in den Lack oder das Lösemittel und Kaltrühron erhielt man frei fließende Dispersionen oder pastenartige Zubereitungen, mit denen man dann in gewünschter Weise die Lacke mattieren konnte. Dieses Verfahren war zeitaufwendig und risikoreich hinsichtlich einer Brandgefahr.In addition to inorganic matting agents, the use of waxes of different compositions for leak matting has been known for many years (Handbook of Nitrocellulose Varnishes, Kraus, Part 2, page 116, Soaps - Oils - Fats - Waxes, 102nd Year No. 6/1976, page 163) . Usually the waxes had to be melted and by incorporating them into the lacquer or the solvent and cold stirrer, free-flowing dispersions or paste-like preparations were obtained, with which the lacquers could then be matted in the desired manner. This process was time consuming and risky in terms of a fire hazard.

Um diese Schwierigkeiten zu umgehen, sind seit einigen Jahren mikronisierte Kohlenwasserstoffwachse im Handel, die sich durch ihre leichte Einarbeitbarkeit ohne Zuhilfenahme von Wärme bewährt haben (Aufsatz "Mattierungsmittel für Lacke" in "Adhäsion", Novemberheft 1977; "Lacke und Lösemittel", Verlag Chemie, Seite 15). Eine Kombination mit Mattierungsmitteln auf anorganischer Basis ist durchaus üblich. Die Erfahrung mit wachsartigen Mottierungsmitteln hat gezeigt, daß besonders Polyethylenrachs-Feinstpulver mit einnr Kornverteilung im Bereich um 10 bis 15 Mikron als Obergrenze die von der Lackindustrie gestellten Anforderungen bestens Erfüllen könnon und in mancher Hinsicht anders zusammengesetzten Mattierungsmitteln überlegon sind. Solche Feinstpulver sind z. B. in der DS-OS 2 713 550 besehrieben. Sie bestehen aus einem ternären Gemisch einos Polyolefinwachses mit einem Esterwachs bzw. einem teilverseiften Esterwachs und einem Diester einer Monocarbonsäure mit einem Diol oder einem Monocarbonsäurediamid und werden durch Versprühen der Uachsschmelzenmischung und anschließende Sichtung auf eine Kornverteilung von 60 bis 80 % zwischen 1 bis 15 Mikron eingestellt.To avoid these difficulties, micronized hydrocarbon waxes have been on the market for a number of years, and have proven themselves due to their ease of incorporation without the aid of heat (essay "Matting agents for paints" in "Adhesion", November issue 1977; "Paints and solvents", Verlag Chemie , Page 15). A combination with matting agents on an inorganic basis is quite common. Experience with wax-like mottling agents has shown that especially high-quality polyethylene vinegar powders with a particle size distribution in the range of 10 to 15 microns as an upper limit can best meet the requirements set by the paint industry and are superior in some respects to matting agents with different compositions. Such very fine powders are e.g. B. described in DS-OS 2,713,550. They consist of a ternary mixture of polyolefin wax an ester wax or a partially saponified ester wax and a diester of a monocarboxylic acid with a diol or a monocarboxylic acid diamide and are adjusted to a particle size distribution of 60 to 80% between 1 to 15 microns by spraying the mixed wax mixture and subsequent screening.

Ein derartiges Verfahren ist technisch aufwendig und damit teuer. Da es andererseits erfahrungsgemäß sehr schwierig ist, Polyolefinwachse durch mechanische Zerkleinerung in einem einzigen Verfahrensschritt in den für die Lackmattierung notwendigen Korngrößenbereich überzuführen [Farbe und Lack, 80. Jahrg., Nr. 4 (1974)], war es Aufgabe der vorliegenden Erfindung, einen weg aufzuzeigen,der zu Feinstpulvern führt, die nicht nur den gewünschten Mattierungseffekt zu erreichen gestatten, sondern darüber hinaus auch leicht in den zu mattierenden Lacken dispergiert werden können und die der so erhaltenen Lackoberfläche einen glatten, samtartigen Griff sowie gute Widerstandsfähigkeit gegen Verkratzen und das sog. "Blankreiben" geben.Such a method is technically complex and therefore expensive. On the other hand, since experience has shown that it is very difficult to convert polyolefin waxes by mechanical comminution in a single process step into the grain size range required for matting the lacquer [Paint and Lacquer, 80th year, No. 4 (1974)], it was the object of the present invention to achieve a way, which leads to very fine powders, which not only allow the desired matting effect to be achieved, but can also be easily dispersed in the lacquer to be matted and which give the lacquer surface thus obtained a smooth, velvety feel and good resistance to scratching and the so-called Give "blank rub".

Überraschenderuuise wurdo gefunden, daß sich Polyolefinwachse dann mühelos bis zur gewünschten Kornfeinheit durch Mahlen zerkleinern lassen, wenn man bei der Mahlung hartes und sprödes Amidwachs zusetzt.Surprisingly, it has been found that polyolefin waxes can then be easily comminuted to the desired fineness by grinding if hard and brittle amide wax is added during the grinding.

Die Erfindung betrifft daher ein Verfahren zur Herstellung eines Lackmattierungsmittels auf Uachsbasis mit einer Korngrößenverteilung von 99 Gew.-%<15 Mikron, welches dadurch gekennzeichnet ist, daß man ein Polyolefinwachs vom durchschnittlichen Molekulargewicht 1 000 bis 9 000 und ein Amidwachs mit einem Fließ-/Tropfpunkt von 130 bis 150°C im Gewichtsverhältnis 90 : 10 bis 10 : 90 einer gemeinsamen Mahlung unterwirft.The invention therefore relates to a process for producing a wax matting agent based on wax with a particle size distribution of 99% by weight <15 microns, which is characterized in that a polyolefin wax with an average molecular weight of 1,000 to 9,000 and an amide wax with a flow / Dropping point of 130 to 150 ° C in a weight ratio of 90: 10 to 10: 90 is subjected to a common grinding.

Sie betrifft des weiteren die nach diesem Verfahren hergestellten Lackmattierungsmittel souie Lacke, die solche Lackmattierungsmittel enthalten.It also relates to the lacquer matting agent souie lacquers produced by this method, which contain such lacquer matting agent.

Nach der erfindungsgemäßen Arbeitsweise gelingt es bei energetisch vertretbarem Aufwand, die geuünschten Feinstpulver mit einer Korngröße von 99 Gew.-% <15 Mikron in - bezogen auf die Einsatzmenge - praktisch quantititativer Ausbeute zu erhalten, ohne daß eine zusätzliche Sichtung erforderlich ist. Dies wer nicht zu erwarten und ist als erheblicher technischer Fortschritt anzusehen.According to the procedure of the invention, it is possible to obtain the desired fine powders with a grain size of 99% by weight <15 microns in practically quantitative yield, based on the amount used, with an economically justifiable effort, without additional screening being necessary. This is not to be expected and is to be seen as a significant technical advance.

Was die Wirksamkeit der erfindungsgemäß hergestellten Feinstpulver betrifft, so stellte sich heraus, daß der Amidwachsanteil in den Lackmattierungsmitteln zwar kaum zur mattierenden Wirkung beiträgt, jedoch überraschenderweise die Einflüsse der Mattierungskomponente auf die Lackoberfläche durch Verbesserung des Gleiteffektes und die daraus resultierende Unempfindlichkeit gegenüber Verkratzungen merklich unterstützt. Dies ließ sich keineswegs vorhersehen. Es mußte vielmehr angenommen werden, daß das Amidwachs lediglich als Mahlhilfsmittel fungiere und seine Anwesenheit zumindest bei höheren Konzentrationen sich eher als nachteilig erweisen würde bezüglich Überstreichbarkeit und Haftung.With regard to the effectiveness of the very fine powders produced according to the invention, it was found that the amide wax content in the matting agents hardly contributes to the matting effect, but surprisingly supports the effects of the matting component on the lacquer surface by improving the sliding effect and the resulting insensitivity to scratches. This was by no means predictable. Rather, it had to be assumed that the amide wax would only function as a grinding aid and that its presence, at least at higher concentrations, would prove to be disadvantageous with regard to paintability and adhesion.

Unter Polyolefinwachsen, die den einen Bestandteil der erfindungsgemäßen Mattierungsmittel darstellon, werden Hnmo- und Copolymerisate des Ethylens, Propylens und Butylens mit Schmelzintervallen im Bereich von 90 bis 140 °C und einem Durchschnittsmolekulargewicht von 1 000 bis 9 000, vorzugsweise 2 000 bis 4 000 verstanden. Bevorzugt sind Ethylen-Propylen-Copolynerisate mit überuiegendem Ethylenantoil.Polyolefin waxes, which are a constituent of the matting agents according to the invention, are monomers and copolymers of ethylene, propylene and butylene with melting intervals in the range from 90 to 140 ° C. and an average molecular weight of 1,000 to 9,000, preferably 2,000 to 4,000 . Ethylene-propylene copolymers with predominant ethylene-tooil are preferred.

Goeignete Amidwachse sind Umsetzungsprodukte technischer Fettsäuren mit 12 bis 34, vorzugsweise 12 bis 18 C-Atomen mit bivalenten aliphatischen Aminen mit 2 bis 6 C-Atomen, wie z. B. Ethylen-, Propylen- und Hexamethylendiamin, die Fließ-/Tropfpunkte von 130 bis 150, vorzugsweise 140 bis 145 °C aufweisen. Ein bevorzugtes Amiduachs ist Di-steaorylethylondiamid.Suitable amide waxes are reaction products of technical fatty acids with 12 to 34, preferably 12 to 18 carbon atoms with bivalent aliphatic amines with 2 to 6 carbon atoms, such as. As ethylene, propylene and hexamethylene diamine, the pour / dropping points from 130 to 150, preferably 140 to 145 ° C. A preferred amiduach is di-steaorylethylondiamide.

Für die gemeinsame Mahlung von Polyolefinwachs und Amidwachs sind beispielsweise Strahlmühlen oder mechanische Mühlen mit integrierter Sichtung geeignet.For the joint grinding of polyolefin wax and amide wax, for example, jet mills or mechanical mills with integrated classifying are suitable.

Bei der Mahlung wird so vorgegangen, daß man die beiden Uachskomponenten in Pulver-, Granulat- oder Schuppenform entweder bereits gemischt oder vorteilhafter nebeneinander der Mühle zuführt. Das Gewichtsverhältnis von Polyolefinwachs zu Amidwachs liegt bei 90 : 10 bis 10 : 90, vorzugsweise bei 70 : 30 bis 30 : 70 und insbesondere bei 60 : 40 bis 40 : 60.The grinding is carried out in such a way that the two wax components in powder, granule or flake form are either already mixed or, advantageously, fed to the mill side by side. The weight ratio of polyolefin wax to amide wax is 90:10 to 10:90, preferably 70:30 to 30:70 and in particular 60:40 to 40:60.

Das erfindungsgemäß gewonnene Feinstpulver läßt sich aufgrund seiner guten Dispergierfähigkeit ohne weiteres mit den üblichen Rührwerken oder Dissolvern kalt in die zu mattierenden Lacksysteme einarbeiten. Je nach gewünschtem Matteffekt, der, wie bereits erwähnt, im wesentlichen durch den Polyolefinwachs-Anteil in der Mischung bestimmt wird, reichen im Falle nicht pigmentierter Lacke Zusätze von 1 bis 4 Gew.-% des pulverförmigen Mattierungsmittels, bezogen auf das Lecksystem, aus. Bei pigmentierten Anstrichstoffen sind höhere Mattierungszusätze notwendig. Eine Vordispergierung in den jeweils angewandten Lösemittoln kann die Verteilung im Lack beschleunigen.Because of its good dispersibility, the fine powder obtained according to the invention can be cold worked into the coating systems to be matted with the usual stirrers or dissolvers. Depending on the desired matt effect, which, as already mentioned, is essentially determined by the proportion of polyolefin wax in the mixture, in the case of unpigmented paints, additions of 1 to 4% by weight of the powdered matting agent, based on the leak system, are sufficient. Higher matting additives are necessary for pigmented paints. Predispersion in the solvents used can accelerate the distribution in the paint.

Die nachstehenden Beispiele dienen der weiteren Erläuterung des Verfahrens und zeigen ferner den Einsatz der Verfahrensprodukte in einigen typischen Lack- bzw. Farbzubereitungen. Die angegebenen Teile sind stets Gewichtsteile.The examples below serve to explain the process further and furthermore show the use of the process products in some typical lacquer or paint preparations. The parts specified are always parts by weight.

Beispiel 1example 1

Einer Gegenstrom-Prallmühle, die aus einer Mahlzone und einem integrierten Windsichter besteht, Werden stündlich 250 kg einer Uachsmischung zugeführt. Die Wachsmischung ist eine grobe 1:1-Mischung aus sprühkonfektioniertem Distearoyl-Ethylendiamid mit Partikelgrößen <400 /u und einem schnittgranulierten Polyethylenwachs (Aufbaupolyethylenuachs vom Molgwicht ca. 3 000, Tropfpunkt 122 bis 127 °C) mit Kantenlängen von 2 bis 4 mm. Die Produktaufgabe erfolgt über eine Dosierschnecke in den Windsichter. Von dort gelangen die Teilchen, die nicht den Feinheitsanforderungen genügen, durch zwei einander gegenüberliegende, mit Druckluft betriebene Injektoren in die Mahlzone. Sie prallen dabei frontal aufeinander und werden dadurch mikronisiert.A counterflow impact mill, which consists of a grinding zone and an integrated wind sifter, is fed with 250 kg of an Uachs mixture per hour. The wax mixture is a rough 1: 1 mixture of spray-finished distearoyl-ethylenediamide with particle sizes <400 / u and a cut-granulated polyethylene wax (build-up polyethylene wax with a molecular weight of approx. 3,000, dropping point 122 to 127 ° C) with edge lengths of 2 to 4 mm. The product is fed into the air classifier via a dosing screw. From there, the particles, which do not meet the fineness requirements, enter the grinding zone through two opposing injectors operated with compressed air. They collide head-on and are thereby micronized.

Das aus der Mühle austretende Mahlgut wird mit der Luftströmung pneumatisch in einen Silo mit einem Belüftungsfilter ausgetragon. Der Druckluftbedarf beträgt bei diesem Durchsatz 34 Nm3/min bei 7 bar und 20 °C. Die Rotordrehzahl des Sichters ist auf 4 000 UpM eingestellt. Nach einer Anfahrzeit von ca. 15 Minuten hat sich im die Mühle verlassenden Mahlgut das 1:1-Mischungsverhältnis der Mahlkomponenten eingestellt. Nach der Coulter Counter Analyse besitzt das gemahlene Produkt eine Gewichtsverteilung von über 99 % kleiner 14 /u und 50 % kleiner 4,5 /u.The ground material emerging from the mill is pneumatically discharged into a silo with a ventilation filter using the air flow. The compressed air requirement at this throughput is 34 Nm 3 / min at 7 bar and 20 ° C. The rotor speed of the classifier is set at 4,000 rpm. After a start-up time of approx. 15 minutes, the 1: 1 mixing ratio of the grinding components has set in the millbase leaving the mill. According to the Coulter Counter Analysis, the ground product has a weight distribution of over 99% less than 14 / u and 50% less than 4.5 / u.

Beisoiel 2Example 2

In eine mechanische Sichtermühle mit vertikaler Achse werden 69 kg/h der in Beispiel 1 verwendeten Uachsmischung über eine Dosierschnecke eingeführt. Die Mühle ist eine Kombination einer Prallschlägermühle mit einem Schaufelradsichtor. Sie ist ausgerüstet mit einem tangentialen Materialeintrag und einem Frischluftonsaugkanal.69 kg / h of the liquid mixture used in Example 1 are introduced into a mechanical classifier mill with a vertical axis via a metering screw. The mill is a combination of a beater mill with a paddle wheel viewer. It is equipped with a tangential material entry and a fresh air intake duct.

Das bei der Mühlendrehzahl von 4 000 UpM-1, der Sichterdrehzahl von 2 200 UpM-]1 und bei einem Luftdurchsatz von 3 100 m3/h aus der Mühle ausgetragene Feingut hat eine Partikelgrößenverteilung von 99,5 % <14,3 /u. Die 50 %-Grenze liegt bei 6,0 /u.The near the mill speed of 4000 rpm -1, the classifier speed of 2200 rpm - m] 1 and with an air throughput of 3100 3 / h from the mill discharged fine material has a particle size distribution of 99.5% <14.3 / u . The 50% limit is 6.0 / u.

Beisbiel 3Example 3

Es wird ein Lackansatz hergestellt aus

  • 15 Gew.-Teilen Kollodiumwolle (feucht), mittelviskos
  • 10 Gew.-Teilen eines Cyclohexanonharzes (Ketonharz N der BASF AG),
  • 8 Gew.-Teilen Dioctylphthalat,
  • 2 Gew.-Teilon Rizinusöl,
  • 35 Gew.-Teilen Butylacetat,
  • 10 Gew.-Teilen n-Butanol,
  • 10 Gew.-Teilen Ethylglykol und
  • 10 Gew.-Teilen Toluol

in welchen man ein nach Beispiel 1 erhaltenes Mattierungsmittel durch 30minutiges Rühren mit 3 000 UpM einarbeitet. Der Lack wird auf Glasplatten in einer Naßfilmstärke von 30 /u aufgetragen. Nach 24stündigem Trocknen mißt man den Mattierungseffekt mit dem Glanzmeßgerät nach Dr. B. Lange.
Figure imgb0001
 A paint batch is made from
  • 15 parts by weight of collodion wool (moist), medium viscosity
  • 10 parts by weight of a cyclohexanone resin (ketone resin N from BASF AG),
  • 8 parts by weight of dioctyl phthalate,
  • 2 parts by weight of castor oil,
  • 35 parts by weight of butyl acetate,
  • 10 parts by weight of n-butanol,
  • 10 parts by weight of ethyl glycol and
  • 10 parts by weight of toluene

in which a matting agent obtained according to Example 1 is incorporated by stirring at 3,000 rpm for 30 minutes. The lacquer is applied to glass plates in a wet film thickness of 30 / u. After drying for 24 hours, measure the matting effect with the gloss meter according to Dr. B. Lange.
Figure imgb0001

Ein Aufpolieren der lackierten Flächen (Belastung 750 g, 100 Bür stenstriche) ist nicht möglich.It is not possible to polish the painted surfaces (load 750 g, 100 brush strokes).

Beispiel 4Example 4

Ein feuchtigkeitshärtender Polyurethanlack mit 42 % Feststoffgehalt (Beckacoat PU 428 der Firma HOECHST AG)wird wie in Beispiel 3 angegeben mit dem nach Beispiel 1 erhaltenen Feinstpulver mattiort.

Figure imgb0002
A moisture-curing polyurethane varnish with a solids content of 42% (Beckacoat PU 428 from HOECHST AG) is matted as indicated in Example 3 with the fine powder obtained according to Example 1.
Figure imgb0002

Der Mattlackfilm ist nicht aufpolierbar.The matt lacquer film cannot be polished.

Beispinel 5Example 5

Ein säurehärtender Lack mit 40 % Feststoffgehalt (Beckurol HP 310 der Firma HOECHSTAG), dem auf 100 Teile Lackansatz als Härter 1 Teil p-Toluolsulfonsäure,gelöst in 19 Teilen n-Butanol, zugefügt werden, wird mit dem Polyethylenwachs-Feinstpulver nach Beispiel 1 mattiert. Die Lackfilme werden wie in Beispiel 3 angegeben geprüft. Sie sind nicht nachpolierbar.An acid-curing paint with a solids content of 40% (Beckurol HP 310 from HOECHSTAG), to which 1 part of p-toluenesulfonic acid, dissolved in 19 parts of n-butanol, is added as a hardener to 100 parts of paint, is matted with the polyethylene wax fine powder according to Example 1 . The paint films are tested as indicated in Example 3. They cannot be polished.

Figure imgb0003
Figure imgb0003

Beispiel 6Example 6

Zur Herstellung eines weiß-pigmentierten Mattlackes kam das Mattisrungsmittel nach Beispiel 2 in folgender Rezeptur zum Einsatz, wobei man das Mattierungsmittel zunächst in die Weißpigmente einmischte, worauf diese Mischung gemeinsam mit dem Binde- und Lösemittel auf einer Trichtermühle abgerieben wurde:

  • 35 Gem.-Teils eines Leinölalkydharzes mit 62 % Öl (Alftalat AL 650 der HOECHST AG),
  • 30 Geu.-Teile Testbenzin,
  • 15 Gew.-Teile Titandioxid,
  • 9 Gew.-Teile gecoatete Kreide (Millicarb der Firma Plüss-Stauffer),
  • 1 Gew.-Teil eines Sikkativs auf Co-Pb-Mn-Basis.
The matting agent according to Example 2 was used in the following recipe to produce a white-pigmented matt varnish, the matting agent first being mixed into the white pigments, after which this mixture was rubbed off together with the binder and solvent on a funnel mill:
  • 35 parts by weight of a linseed oil alkyd resin with 62% oil (Alftalat AL 650 from HOECHST AG),
  • 30 parts by weight white spirit,
  • 15 parts by weight of titanium dioxide,
  • 9 parts by weight of coated chalk (Millicarb from Plüss-Stauffer),
  • 1 part by weight of a desiccant based on Co-Pb-Mn.

Die Prüfung der Lackfilme erfolgte wie in Beispiel 3 angageben. Die Filme sind nicht nachpolierbar.

Figure imgb0004
The coating films were tested as indicated in Example 3. The films cannot be polished.
Figure imgb0004

Claims (6)

1. Verfahren zur Horstellung eines Lackmattierungsmittels auf Wachsbasis mit einer Korngrößenverteilung von 99 Gew.-% <15 Mikron, dadurch pekennzeichnet, daß man ein Polyolefinwachs vom durchschnittlichen Molekulargewicht 1 000 bis 9 000 und ein Amidwachs mit einem Fließ-/Tropfpunkt von 130 bis 150 ]°C im Gewichtsverhältnis 90 : 10 bis 10 : 90 einer gemeinsamen Mahlung unterwirft. 1st A process for producing a wax-based paint matting agent with a particle size distribution of 99% by weight <15 microns, characterized in that a polyolefin wax with an average molecular weight of 1,000 to 9,000 and an amide wax with a pouring / dropping point of 130 to 150 ° C in a weight ratio of 90:10 to 10:90 is subjected to a common grinding. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Amidwachs das Umsetzungsprodukt aus einer Fettsäure mit 12 bis 34 C-Atomen und einem bivalenten aliphatischen Amin mit 2 bis 6 C-Atomen ist.2. The method according to claim 1, characterized in that the amide wax is the reaction product of a fatty acid having 12 to 34 carbon atoms and a bivalent aliphatic amine having 2 to 6 carbon atoms. 3. Lackmattierungsmittel auf Uachsbasis, welches aus 10 bis 90 Gew.-% eines Polyolefinwachsos vom mittleren Molekulargewicht 1 000 bis 9 000 und 90 bis 10 Gew.-% eines Amidwachses besteht und ein homogenes Feinstpulver mit einer Korngrößenverteilung von 99 Gew.-% <15 Mikron darstellt, erhalten nach Anspruch 1.3. Lacquer matting agent based on wax, which consists of 10 to 90% by weight of a polyolefin wax of average molecular weight 1,000 to 9,000 and 90 to 10% by weight of an amide wax and a homogeneous fine powder with a particle size distribution of 99% by weight < 15 microns, obtained according to claim 1. 4. Verwendung von Amidwachsen aus einer Fettsäure mit 12 bis 34 C-Atomen und einem bivalenten aliphatischen Amin mit 2 bis 6 C-Atomen als Hilfsmittel bei der Mahlung von Polyolefinwachs vom mittleren Molgewicht 1 000 bis 9 000 zu einem Feinstpulver mit einer Korngrößenvsrteilung von 99 Gew.-%<15 Mikron für die Lackmattierung.4.Use of amide waxes from a fatty acid with 12 to 34 carbon atoms and a bivalent aliphatic amine with 2 to 6 carbon atoms as an aid in the grinding of polyolefin wax with an average molecular weight of 1,000 to 9,000 to a very fine powder with a particle size distribution of 99 % By weight <15 microns for paint matting. 5. Verwendung nach Anspruch 4, dadurch gekennzeichnet, daß das Gewichtsverhältnis Polyolefinwaichs : Amidwachs 90 : 10 bis 10 : 90 beträgt.5. Use according to claim 4, characterized in that the weight ratio of polyolefin wax: amide wax is 90:10 to 10:90. 6. Mattlacke, die ein nach Anspruch 1 hergestelltes Mattierungsmittel enthalten.6. matt lacquers containing a matting agent prepared according to claim 1.
EP80106157A 1979-10-20 1980-10-10 Matting agent for varnishes based on wax, process for its production, and matted varnishes Expired EP0028713B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2942487 1979-10-20
DE19792942487 DE2942487A1 (en) 1979-10-20 1979-10-20 WATER-BASED VARNISH MATERIAL AND METHOD FOR THE PRODUCTION THEREOF

Publications (2)

Publication Number Publication Date
EP0028713A1 true EP0028713A1 (en) 1981-05-20
EP0028713B1 EP0028713B1 (en) 1982-04-28

Family

ID=6083981

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80106157A Expired EP0028713B1 (en) 1979-10-20 1980-10-10 Matting agent for varnishes based on wax, process for its production, and matted varnishes

Country Status (10)

Country Link
US (1) US4342602A (en)
EP (1) EP0028713B1 (en)
JP (1) JPS5665056A (en)
AT (1) ATE925T1 (en)
AU (1) AU535631B2 (en)
BR (1) BR8006707A (en)
DE (2) DE2942487A1 (en)
ES (1) ES495922A0 (en)
MX (1) MX155639A (en)
ZA (1) ZA806393B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0324077A3 (en) * 1988-01-15 1991-05-29 Hüls Aktiengesellschaft Additive for printing inks and paints, and method of making it
WO2003104330A1 (en) * 2002-06-05 2003-12-18 Clariant Gmbh Mixtures of finely ground waxes
US8563134B2 (en) 2009-03-19 2013-10-22 Clariant Finance (Bvi) Limited Usage of copolymerisates as additives for lacquers

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4614674A (en) * 1984-05-11 1986-09-30 Ciba-Geigy Corporation Powder coating compositions for the preparation of matt coatings
JPS61143595A (en) * 1984-12-17 1986-07-01 Honny Chem Ind Co Ltd Formation of electrodeposited mat paint film
DE3531123A1 (en) * 1985-08-31 1987-03-12 Schramm Lacke Gmbh METHOD FOR PAINTING RAILWAY OR TABLED SUBSTRATE MATERIALS
US5017222A (en) * 1989-12-07 1991-05-21 Dow Corning Corporation Polish containing micronized wax particles
US6829654B1 (en) 2000-06-23 2004-12-07 Cloudshield Technologies, Inc. Apparatus and method for virtual edge placement of web sites
EP1656340B1 (en) * 2003-08-12 2012-07-18 Boehringer Ingelheim International GmbH Processes for making 1-carbamoylcycloalkylcarboxylic acid compounds
US7341619B2 (en) * 2004-11-23 2008-03-11 Chevron Phillips Chemical Company, Lp Olefin waxes having improved hardness or viscosity
US7527686B2 (en) * 2004-11-23 2009-05-05 Chevron Phillips Chemical Company, Lp Olefin waxes having improved hardness or viscosity
DE102010052028B4 (en) 2010-11-23 2025-05-15 Sasol Germany Gmbh Process for grinding waxes using grinding aids in a jet mill, use of polyols as grinding aids and wax powder containing polyols
US11795332B2 (en) * 2019-05-17 2023-10-24 Honeywell International Inc. Coatings containing micronized polymers as matting agents

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2113990A1 (en) * 1970-04-17 1971-11-04 Leuna Werke Veb Modified ketone-aldehyde resins primers,lacquers
DE2601602A1 (en) * 1976-01-17 1977-07-21 Basf Ag Atomisation of waxes partic. polyolefins - by 8pplication of a high electric potential to a melt and transfer to earthed plate

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE647416C (en) * 1935-12-03 1937-07-03 Ernst Ludwig Marx Process for the production of clear, matt-drying nitrocellulose lacquers
US2433833A (en) * 1944-11-24 1948-01-06 Auer Laszlo Flatting agent and process for making same
BE597186A (en) * 1959-11-19
US3441628A (en) * 1965-12-13 1969-04-29 Leuna Werke Veb Process for producing waxlike low molecular ethylene polymers and copolymers
DE2713550C2 (en) 1977-03-28 1983-08-11 Basf Ag, 6700 Ludwigshafen Paint matting agents

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2113990A1 (en) * 1970-04-17 1971-11-04 Leuna Werke Veb Modified ketone-aldehyde resins primers,lacquers
DE2601602A1 (en) * 1976-01-17 1977-07-21 Basf Ag Atomisation of waxes partic. polyolefins - by 8pplication of a high electric potential to a melt and transfer to earthed plate

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0324077A3 (en) * 1988-01-15 1991-05-29 Hüls Aktiengesellschaft Additive for printing inks and paints, and method of making it
WO2003104330A1 (en) * 2002-06-05 2003-12-18 Clariant Gmbh Mixtures of finely ground waxes
US8563134B2 (en) 2009-03-19 2013-10-22 Clariant Finance (Bvi) Limited Usage of copolymerisates as additives for lacquers

Also Published As

Publication number Publication date
ES8105372A1 (en) 1981-06-16
ATE925T1 (en) 1982-05-15
AU6350980A (en) 1981-04-30
BR8006707A (en) 1981-04-22
MX155639A (en) 1988-04-08
ZA806393B (en) 1981-10-28
AU535631B2 (en) 1984-03-29
EP0028713B1 (en) 1982-04-28
JPS6359431B2 (en) 1988-11-18
DE2942487A1 (en) 1981-04-30
JPS5665056A (en) 1981-06-02
US4342602A (en) 1982-08-03
DE3060343D1 (en) 1982-06-09
ES495922A0 (en) 1981-06-16

Similar Documents

Publication Publication Date Title
DE69504335T2 (en) METAL LEAF-CONTAINING AQUEOUS DISPERSION COLOR FOR VEHICLES
EP1756234B1 (en) Aqueous coating composition with corrosion resistant thin-coat aluminium pigments method for production and use therof
DE69408267T2 (en) Process for the preparation of a powder coating composition
DE3752320T2 (en) Powder coating based on polyvinylidene fluoride
EP0028713B1 (en) Matting agent for varnishes based on wax, process for its production, and matted varnishes
DE10204304A1 (en) pigment granules
DE2737737A1 (en) WATER DISPERSIBLE DRY PIGMENT COMPOUNDS AND METHOD FOR THEIR PRODUCTION
DE10361437A1 (en) Metal pigments with crosslinkable binder coating, coating composition, process for the preparation of the coated metal pigments and their use
WO2003066743A1 (en) Pigment preparations
WO1999065995A1 (en) Pigment preparation
EP2157138A1 (en) Thin, platy iron pigments, method for their manufacture and use
EP0195931A1 (en) Water dilutable coating compositions for base coats for wet-on-wet application of clear coat on base coat
EP1483336B2 (en) Method for the production of coated, fine-particle, inorganic solids and use thereof
DE2263049A1 (en) HEAT-RESISTANT ACRYLIC POLYMER POWDER COATING COMPOSITIONS
EP0222061A2 (en) Process for preparing micronized waxes
DE202018007002U1 (en) Aqueous composition and aqueous coating agent
EP0027997A1 (en) Mineral filler, particularly calcium carbonate for paints and paper coatings
DE3112659A1 (en) METHOD FOR PRODUCING AQUEOUS VARNISHES
DE3783781T2 (en) AQUEOUS COATING COMPOSITION CONTAINING FINE PARTICLES FROM A SOLUTION OF A WATER-INSOLUBLE RESIN.
DE69201600T2 (en) Resin composition for powder coatings.
WO2011141131A1 (en) Coating powders and use thereof
DE154679T1 (en) NAIL POLISHES AND METHOD FOR THE PRODUCTION THEREOF.
DE2713550C2 (en) Paint matting agents
DE2521361A1 (en) PROCESS FOR THE PRODUCTION OF MATTING AGENTS FOR LACQUERS
EP0324077A2 (en) Additive for printing inks and paints, and method of making it

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Designated state(s): AT BE CH DE FR GB IT NL SE

17P Request for examination filed

Effective date: 19810327

ITF It: translation for a ep patent filed
GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Designated state(s): AT BE CH DE FR GB IT NL SE

REF Corresponds to:

Ref document number: 925

Country of ref document: AT

Date of ref document: 19820515

Kind code of ref document: T

REF Corresponds to:

Ref document number: 3060343

Country of ref document: DE

Date of ref document: 19820609

ITTA It: last paid annual fee
EAL Se: european patent in force in sweden

Ref document number: 80106157.3

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: CH

Payment date: 19970925

Year of fee payment: 18

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 19971002

Year of fee payment: 18

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 19971031

Year of fee payment: 18

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19981010

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19981011

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19981031

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19981031

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 19990325

Year of fee payment: 19

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

EUG Se: european patent has lapsed

Ref document number: 80106157.3

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 19990922

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19990923

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 19990924

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 19990928

Year of fee payment: 20

BE20 Be: patent expired

Free format text: 20001010 *HOECHST A.G.

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000801

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20001009

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20001010

REG Reference to a national code

Ref country code: GB

Ref legal event code: PE20

Effective date: 20001009

NLV7 Nl: ceased due to reaching the maximum lifetime of a patent

Effective date: 20001010

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT